Chloromethyl Methyl Ether → 1-[2-Hydroxy-4,6-bis(methoxymethoxy)phenyl]ethanone
반응식
[OH:1][C:2]1[CH:7]=[C:6]([OH:8])[CH:5]=[C:4]([OH:9])[C:3]=1[C:10](=[O:12])[CH3:11].C(N(CC)C(C)C)(C)C.[CH3:22][O:23][CH2:24]Cl.[O:26]1[CH2:30]CC[CH2:27]1>>[OH:1][C:2]1[CH:7]=[C:6]([O:8][CH2:22][O:23][CH3:24])[CH:5]=[C:4]([O:9][CH2:27][O:26][CH3:30])[C:3]=1[C:10](=[O:12])[CH3:11]참가 물질
실험 절차
In 200 ml of anhydrous tetrahydrofuran were dissolved 30 g of 2',4',6'-trihydroxyacetophenone and 115.0 g of N,N-diisopropylethylamine, and 50.2 g of chloromethyl methyl ether was gradually added to the solution under ice cooling over a period of 20 minutes and the reaction mixture was stirred under ice cooling for 1 hour and at room temperature for 4 hours to effect reaction. After the reaction, the reaction mixture was extracted with 3 l of ether, and the ether layer was washed with water (500 ml×3 times), shaken with a saturated aqueous solution of sodium chloride (300 ml×2 times), dried with anhydrous sodium sulfate, and filtered. The solvent was removed from the filtrate by distillation and the obtained residue was recrystallized from a mixed solvent of methanol and water to obtain 18.9 g (yield=41.4%) of 2'-hydroxy-4',6'-bis(methoxymethoxy)acetophenone in the form of a colorless prism.
후처리
- additionwas gradually added to the solution under ice cooling over a period of 20 minutes
- customreaction
- customAfter the reaction
- extractionthe reaction mixture was extracted with 3 l of ether
- washthe ether layer was washed with water (500 ml×3 times)
- stirringshaken with a saturated aqueous solution of sodium chloride (300 ml×2 times)
- dry with materialdried with anhydrous sodium sulfate
- filtrationfiltered
- customThe solvent was removed from the filtrate by distillation
- customthe obtained residue was recrystallized from a mixed solvent of methanol and water
출처 및 근거
- ORD 기록
- ord-3d2d469332b34b23b5b5333bdf6b4cdc
- 출처 데이터셋
- uspto-grants-1993_08
- 특허 번호
- US05234951
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